CN108745299A - A kind of preparation method of special appearance adsorbent - Google Patents

A kind of preparation method of special appearance adsorbent Download PDF

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Publication number
CN108745299A
CN108745299A CN201810472060.1A CN201810472060A CN108745299A CN 108745299 A CN108745299 A CN 108745299A CN 201810472060 A CN201810472060 A CN 201810472060A CN 108745299 A CN108745299 A CN 108745299A
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Prior art keywords
adsorbent
special appearance
preparation
stand
solution
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CN201810472060.1A
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Inventor
张凤荣
张作芳
韩丹丹
汪涛
郭燕风
李明君
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Heze University
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Heze University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Medicinal Preparation (AREA)

Abstract

The present invention relates to adsorbent preparing technical fields, and in particular to a kind of preparation method of special appearance adsorbent includes the following steps:(1)It weighs a certain amount of polysaccharide to be dissolved into the aqueous solution of acid, stirring is then allowed to stand 1 ~ 5 h until polysaccharide dissolving;(2)Under stiring, by step(1)In polysaccharide solution with 1 ~ 2 drop/2 s be added drop-wise in the mixed solution of certain density sodium hydroxide and ethyl alcohol, be then allowed to stand 1 ~ 12 h;(3)Step(2)In mixed liquor filtering, washing to neutrality is to get to special appearance adsorbent.Adsorbent prepared by the present invention has the special appearance of stoning hawthorn shape, has larger specific surface area, there is ideal treatment effect to the waste water containing heavy metal ion and dyestuff;Preparation process is simple, mild condition.

Description

A kind of preparation method of special appearance adsorbent
Technical field
The present invention relates to adsorbent preparing technical fields, and in particular to a kind of preparation method of special appearance adsorbent.
Background technology
In recent years, the pollution of global freshwater resources is one of main Environmental Problems of facing mankind, especially heavy metal and The pollution of organic matter causes the extensive concern of people.With petrochemical industry, printing, dyeing, weaving, plastics, leather, food etc. The fast development of industry, the industrial wastewater containing organic dyestuff and heavy metal are discharged into soil and water body in large quantities, seriously Threaten the living space of the mankind.In addition, being limited, research water money due to facilitating the freshwater resources total amount utilized for the mankind Recycling for source has very important significance.However, with the continuous growth of population, global freshwater resources consumption increases Long speed is increased with the rate of population increase more than twice, it means that the consumption of every 20 years global freshwater resources will turn over One times.In order to ensure the supply of freshwater resources, reduces water pollution or the processing recycling of polluted source is received each National more and more attention.
Currently, the industrial wastewater of processing heavy metal and organic dyestuff mainly has chemical method, physical-chemical process and biotechnology The methods of.In these processing methods, absorption method has high treating effect, easy to operate and good selective, especially Have pollution is strong, low concentration, other processing methods are difficult to the heavy metal pollution being effectively treated and organic polluting water field Special application value.The active charcoal of common adsorbent, zeolite, clay, biopolymer, molecular sieve and some industrial wastes Object etc., but these adsorbent prices are high, adsorption capacity is low.
Chitosan be one kind be present in nature it is renewable, have no toxic side effect, biocompatibility and degradability it is good Native amino the polysaccharide ,-NH contained in structure2There is stronger combination to metal ion with-OH groups.Using Chitosan microball or chitosan film, can effectively in Adsorption waste water low-concentration heavy metal ions and waste water from dyestuff color. But most of nano adsorbers, all exist with pulverulence, it is small there are specific surface area the problems such as, limit its practical application.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation methods of special appearance adsorbent, prepare Go out the adsorbent of the stoning hawthorn shape of large specific surface area.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:A kind of special appearance absorption The preparation method of agent, includes the following steps:
(1)It weighs a certain amount of polysaccharide to be dissolved into the aqueous solution of acid, stirring is then allowed to stand 1 ~ 5 h until polysaccharide dissolving;
(2)Under stiring, by step(1)In polysaccharide solution with 1 ~ 2 drop/2 s be added drop-wise to certain density sodium hydroxide and second In the mixed solution of alcohol, it is then allowed to stand 7 ~ 17 h;
(3)Step(2)In mixed liquor filtering, washing to neutrality is to get to special appearance adsorbent.
Preferably, the step(1)In polysaccharide be one kind in chitosan or xanthans or ammonium alginate, institute It is one kind in citric acid or acetylacetone,2,4-pentanedione or ethylenediamine tetra-acetic acid or acetic acid to state acid.
Preferably, the step(1)The middle solution left standstill time is 2 h.
Preferably, the step(2)The rate of addition of middle polysaccharide solution is 1/2 s of drop.
Preferably, the step(2)The mass concentration of middle sodium hydroxide is 10%.
Preferably, the step(2)The volumetric concentration of middle ethyl alcohol is 20%.
Preferably, the step(2)The time of repose of middle mixed liquor is 12 h.
Preferably, the step(3)Middle gained special appearance adsorbent is stoning hawthorn shape adsorbent.
Compared with prior art, the beneficial effects of the invention are as follows:Adsorbent prepared by the present invention has stoning hawthorn shape Special appearance has larger specific surface area, there is ideal treatment effect to the waste water containing heavy metal ion and dyestuff; Preparation process of the present invention is simple, mild condition.
Description of the drawings
Fig. 1 is that special appearance adsorbent prepared by embodiment 1 is schemed through NaCl solution treated mapping;
Fig. 2 is photo before and after special appearance adsorbent absorption fuchsin solution prepared by embodiment 1.
Specific implementation mode
Embodiment described here is some preferred implementation methods, for further describing and demonstrating the present invention, it is not intended to Limit the invention to the details of following determinations.
Embodiment 1:
(1)It weighs 10 g chitosans and is dissolved into 500 ml 5%(v/v)In acetum, mechanical agitation is until chitosan dissolves, so After stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In chitosan solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor by the acidproof filter-cloth filtering of 150 mesh, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml fuchsin solution(w t=0.01%)In, it is inhaled It is attached, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 2:
(1)It weighs 10 g xanthans and is dissolved into 500 ml 5%(v/v)In acetum, mechanical agitation is until xanthans dissolves, so After stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In xanthan gum solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml rhodamine b solution(w t=0.01%)In, it carries out Absorption, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 3:
(1)It weighs 10 g sodium alginates and is dissolved into 500 ml 5%(v/v)In acetum, mechanical agitation is until sodium alginate is molten Solution, is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In sodium alginate soln with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml Coomassie Brillant Blue solutions(w t=0.01%)In, It is adsorbed, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 4:
(1)It weighs 10 g chitosans and is dissolved into 500 ml 5%(v/v)In citric acid solution, mechanical agitation is dissolved up to chitosan, It is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In chitosan solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml fuchsin solution(w t=0.01%)In, it is inhaled It is attached, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 5:
(1)It weighs 10 g chitosans and is dissolved into 500 ml 5%(v/v)In edta solution, mechanical agitation is until shell is poly- Sugar dissolving, is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In chitosan solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml fuchsin solution(w t=0.01%)In, it is inhaled It is attached, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 6:
(1)It weighs 10 g chitosans and is dissolved into 500 ml 5%(v/v)In acetylacetone,2,4-pentanedione solution, mechanical agitation is until chitosan is molten Solution, is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In chitosan solution 800 ml are added drop-wise to the speed of 1 drop/2s Sodium hydroxide(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml fuchsin solution(w t=0.01%)In, it is inhaled It is attached, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 7:
(1)It weighs 10 g xanthans and is dissolved into 500 ml 5%(v/v)In citric acid solution, mechanical agitation is dissolved up to xanthans, It is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In xanthan gum solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml rhodamine b solution(w t=0.01%)In, it carries out Absorption, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 8:
(1)It weighs 10 g xanthans and is dissolved into 500 ml 5%(v/v)In edta solution, mechanical agitation is until xanthan Peptization solution is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In xanthan gum solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml rhodamine b solution(w t=0.01%)In, it carries out Absorption, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 9:
(1)It weighs 10 g xanthans and is dissolved into 500 ml 5%(v/v)In acetylacetone,2,4-pentanedione solution, mechanical agitation is until xanthan peptization Solution, is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In xanthan gum solution with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml rhodamine b solution(w t=0.01%)In, it carries out Absorption, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 10:
(1)It weighs 10 g sodium alginates and is dissolved into 500 ml 5%(v/v)In citric acid solution, mechanical agitation is until sodium alginate Dissolving, is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In sodium alginate soln with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml Coomassie Brillant Blue solutions(w t=0.01%)In, It is adsorbed, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 11:
(1)It weighs 10 g sodium alginates and is dissolved into 500 ml 5%(v/v)In edta solution, mechanical agitation is until sea Mosanom dissolves, and is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In sodium alginate soln with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml Coomassie Brillant Blue solutions(w t=0.01%)In, It is adsorbed, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.
Embodiment 12:
(1)It weighs 10 g sodium alginates and is dissolved into 500 ml 5%(v/v)In acetylacetone,2,4-pentanedione solution, mechanical agitation is until alginic acid Sodium dissolves, and is then allowed to stand 2 h.
(2)It under magnetic stirring, will with syringe(1)In sodium alginate soln with 1 drop/2 s speed be added drop-wise to 800 Ml sodium hydroxides(10w t%)And ethyl alcohol(20%(v/v))Mixed liquor in, be then allowed to stand 12 h.
(3)?(2)In mixed liquor be sieved through filter by 150 mesh stainless steels, with water washing three times to neutrality, obtain stoning mountain Short, bristly hair or beard shape adsorbent.
(4)It weighs 0.05 g stoning hawthorn shape adsorbents and is added to 50 ml Coomassie Brillant Blue solutions(w t=0.01%)In, It is adsorbed, the results showed that, after adsorbing 3 h, percent of decolourization is up to 98% or more.

Claims (8)

1. a kind of preparation method of special appearance adsorbent, which is characterized in that include the following steps:
(1)It weighs a certain amount of polysaccharide to be dissolved into the aqueous solution of acid, stirring is then allowed to stand 1 ~ 5 h until polysaccharide dissolving;
(2)Under stiring, by step(1)In polysaccharide solution with 1 ~ 2 drop/2 s be added drop-wise to certain density sodium hydroxide and second In the mixed solution of alcohol, it is then allowed to stand 7 ~ 17 h;
(3)Step(2)In mixed liquor filtering, washing to neutrality is to get to special appearance adsorbent.
2. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(1)In Polysaccharide is one kind in chitosan or xanthans or sodium alginate, and the acid is citric acid or acetylacetone,2,4-pentanedione or ethylenediamine tetra-acetic acid Or one kind in acetic acid.
3. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(1)In it is molten Liquid time of repose is 2 h.
4. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(2)In it is more The rate of addition of sugar juice is 1/2 s of drop.
5. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(2)Middle hydrogen The mass concentration of sodium oxide molybdena is 10%.
6. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(2)Middle second The volumetric concentration of alcohol is 20%.
7. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(2)In mix The time of repose for closing liquid is 12 h.
8. the preparation method of special appearance adsorbent according to claim 1, it is characterised in that:The step(3)Middle institute It is stoning hawthorn shape adsorbent to obtain special appearance adsorbent.
CN201810472060.1A 2018-05-17 2018-05-17 A kind of preparation method of special appearance adsorbent Pending CN108745299A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1417133A (en) * 2002-10-28 2003-05-14 陆娴婷 Water purifying agent and its prepn process
CN102553542A (en) * 2012-02-17 2012-07-11 杭州师范大学 Granular absorbent with nano-apertures and preparation method for granular absorbent
CN102580690A (en) * 2012-03-06 2012-07-18 杭州师范大学 Nano-aperture granular adsorbent and preparation and application thereof
CN103071460A (en) * 2013-01-09 2013-05-01 中科院广州化学有限公司 Chitosan crosslinking adsorbent as well as preparation method and application thereof
CN103127913A (en) * 2012-11-12 2013-06-05 武汉斯隆电气有限公司 Nanoscale adsorbent used for treating micropollutants in water

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1417133A (en) * 2002-10-28 2003-05-14 陆娴婷 Water purifying agent and its prepn process
CN102553542A (en) * 2012-02-17 2012-07-11 杭州师范大学 Granular absorbent with nano-apertures and preparation method for granular absorbent
CN102580690A (en) * 2012-03-06 2012-07-18 杭州师范大学 Nano-aperture granular adsorbent and preparation and application thereof
CN103127913A (en) * 2012-11-12 2013-06-05 武汉斯隆电气有限公司 Nanoscale adsorbent used for treating micropollutants in water
CN103071460A (en) * 2013-01-09 2013-05-01 中科院广州化学有限公司 Chitosan crosslinking adsorbent as well as preparation method and application thereof

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